Reaktion #40490

ord-7898338d32e44508a9b26d36d2f6cd9f

Reaktionsbedingungen

Temperatur
130°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturto cool to room temperature
  2. 2
    SonstigeThe precipitated yellow solids were removed by filtration
  3. 3
    Waschenwashed with water, 2×5 ml

Vorschrift

Crude 2-benzoyl-6-chloro-1,2,3,9-tetrahydro-β-carbolin-4-one (4 g) was dissolved in 30 ml of anhydrous hydrazine and stirred at reflux (130° C. oil bath) under N2 for 6 hours, after which the reaction mixture was allowed to cool to room temperature and sit overnight. The precipitated yellow solids were removed by filtration and washed with water, 2×5 ml, to yield 785 mg (30%) of 4-amino-6-chloro β-carboline as an off white solid. Additional water was added to the combined filtrates until no further precipitation occurred. These solids were also removed by filtration to give 1.056 g (39%) of 4-amino-6-chloro β-carboline as yellow solids, (69% total yield).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07727985B2uspto-grants-2010_06